Method for the digestion of cellulose-bearing material



W. E. SEGL March 30, 1954 METHOI?` FOR THE DIGESTION OF` CELLULOSE-BEARING MATERIAL Filed 0G12. 27. 1951 2 Sheets-Sheet 1 ls/ MCL FIG.|

WALTER E. sEGl.

INVENTOR,

AGENT.

March 30, 1954 w. E. sEGL METHOD FOR THE DIGEsTioN oF cELLULosE-BEARTNG MATERIAL Filed oct. 27. 1951 2 Sheets-Sheet 2 FIC-3.2

FIG.4

FIG.3

WALT E R E. SEGL INVENTOR.

AGENT.

Patented Mar. 30, 1954 METHOD FDR THE DIGESTION F CELLULOSE-BEARING MATERIAL Walter E. Segl, Wilmington, Del., assigner to Hercules Powder Company, Wilmington, Del., a corporation of Delaware Application October 27, 1951, Serial No. 253,521

9 Claims. l

This invention relates to the purification of cellulose-bearing materials and more particularly to improvements in the art of digestion of such materials with chemicals at elevated temperatures and pressures.

This invention is a continuation-in-part of my copending application, Serial No. 104,616, filed- July 14, 1949.

There are numerous factors to be considered in the processing of cellulose-bearing materials to render them satisfactory for ultimate predetermined use. Additionally, the ultimate predetermined use of the cellulose imposes requirements upon the method and apparatus utilized for treatment which requirements have heretofore not been satisfied. For example, if it is desired to manufacture a purified or semichemical pulp from wood, fibrous or other similar cellulose-bearing material or if it is desired to manufacture chemical cellulose from cotton linters or the like, the physical structure and form of the starting material will vary widely and the method and apparatus must be possessed of great versatility to accommodate variation in physical form, chemicals, temperatures and pressures. Moreover, the method and apparatus utilized for a substantially continuous digestion should be capable of handling the material to be treated with a minimum of pretreatment and a minimum of subsequent treatment to render the material uniform and satisfactory for end product use.

Therefore, an object of the present invention is to provide a method for the substantially continuous digestion of cellulose-bearing material and particularly cotton linters in which a material of uniform quality is obtained.

It is another object of the invention to provide a method for rapid purification of cellulosebearing material by high-consistency digestion.

It is still another object of the invention to provide an improved method for minimizing pretreatment and subsequent treatment and affording rapid purification of the cellulose with uniform viscosity and quality characteristics.

It is a further object of this invention to provide a novel method and apparatus for forming and disintegrating pressure-resistant compacts of cellulose-bearing material. A

Other objects of the invention will be apparent hereinafter with reference to the following description and the appended claims.

Generally described, they present invention comprises a method for the digestion of a cellulose-bearing material which comprises wetting into a pressure-resistant compact.

the material with liquid, removing a portion of the liquid, forming a pressure-resistant compact of the material, digesting material from the compact in the presence of digestion medium and under superatmospheric pressure and temperature, and subjecting the digested material to reduced pressure at intermittent intervals.

In a particular aspect the present invention is primarily concerned with a method and apparatus for forming and disintegratng a pressure-resistant compact of cellulose-bearing material.

An example of the general operation of the invention is given. The cellulosic starting material is subjected to the usual preparation treatment. For example, Wood, straw, and other bulk cellulose-containing materials are reduced to chips or shreds and screened. Preferably, the chips or like material to be treated will have at least one thickness in the order of 1/4 inch and will pass a, 1x1-inch mesh screen. Raw linters and similar fibrous cellulosic material are simply subjected to the usual bale opening facilities. Ground wood pulp or chemical wood pulp may be used without additional preparation where in the former instance substantially complete digestion is desired and in the latter further digestion treatment for special end product use. The cellulosic starting material after suitable preparation, if necessary, is then weighed by a constant weight feed device and a pretreatment solution of water or water and chemicals is thoroughly mixed with the material in a pretreatment zone. The pretreatment solution may be water to serve as a lubricant for the wetted material, or it may be water and chemicals in which the latter may be acid or alkaline digestion medium, with or without wetting agent, detergent, or other digestion aid or bleaching medium, or like chemical agents. These chemicals may be employed as desired to effect certain desired conditioning prior to actual digestion. An excess of the pretreatment solution should be present to insure positive wetting of the material and adequate lubrication. Ihe material from the pretreatment zone is continuously passed into a compaction zone wherein excess pretreatment solution is squeezed from the material as it is formed The material from the pressure-resistant compact is continuously fed into the digestion zone in the presence of digestion chemicals and under conditions of superatmospheric pressure and temperature. The quantity and type of chemicals used, the pressure and temperature, and length of the digestion period may be varied according to the yield and quality of the cellulose desired. The material is then continuously passed from the digestion zone into a second compaction zone wherein the excess digestion chemicals are squeezed from the material as it is formed into a compact. 'I'he material from the compact is then blown to substantially atmospheric pressure at intermittent intervals whereby the formerly compacted material is thoroughly disintegrated and is free of small lumps or pills. The intervals at which the material is blown to substantially atmospheric pressure are regulated and are of short duration to afford a small and carefully controlled pressure drop in the digestion zone. The discharged material may then be washed, bleached, sheeted, or bulk dried, or otherwise suitably processed as desired for subsequent use.

A preferred embodiment of the invention has been chosen for purposes of illustration and description and is shown in the accompanying diagrammatic drawings forming a part of the specication wherein reference symbols refer to like parts wherever they occur.

Fig. l is a diagrammatic ow sheet depicting a method and suitable apparatus for effecting the digestion of cellulose-bearing material.

Fig. 2 is an enlarged sectional view of a portion of the flow diagram in Fig. l depicting the method for forming and disintegrating compacts of cellulose-bearing material wherein the face of the ram is curved convexly.

Fig. 3 is an enlarged View depicting an initial stage in the formation of the pressure-resistant compact lof cellulose-bearing material wherein as an alternative embodiment the face of the ram is flat.

Fig. fi is an enlarged view depicting the forniation of the pressure-resistant compact initially illustrated in Fig. 3.

Fig. 5 is an enlarged view depicting an initial stage in the disintegration of the pressure-resistant compact initially illustrated in Fig. 3.

Fig. 6 is an enlarged view depicting the disintegration of the pressure-resistant compact initially illustrated in Fig. 3.

In the presentation of the preferred embodiment of the invention, raw cotton linters are used as an example of the material. being processed and pressure is given in pounds per square inch gage, temperature in degrees F., and parts and percentages by weight.

Referring now to Fig. l of the accompanying drawings, 1 part of linters and 6 parts of solution were continuously charged through lines I and 2, respectively, into a conduit 3. The linters contained about 6% moisture andthe solution was a normal aqueous digestion solution, containing 2.5% caustic alkali and detergent, heated to 180. From the conduit 3, the material was continuously charged into a pretreatment zone 4 in lpressureresistant compact by which it was thoroughly mixed and wetted. The

gressed. The blow-out vent additionally serves as a release to atmosphere if accidental back 4 pressure occurs. From the pretreatment zone 5, the material was continuously charged through conduit 9 into a first compaction zone it in which more than of the solution was removed and the material was formed into a pressure-resistant compact. The compaction zone II! contained a motor-driven screw Il disposed in a foraminous jacket I2 through which the excess solution passed as the material was compacted by the screw. The excess solution was removed from the compaction zone It through line it as the material was continuously formed .into the being forced through conduit 42 and then against a pressureactuated ram I4 in compact disintegrating zone 43. The ram I4 was provided with a valved air line I5 for controlling the amount of force dein/- ered by the ram against the pressure-resistant compact. rl"he ram additionally serves as a check Valve for the compaction zone in the event the pressure-resistant compact should fail to withstand the fiuid pressure within the system. The material was continuously extruded against the head of ram I4 where it was disintegrated by the continuous and directly opposed compressive force and dropped therefrom into a digestion zone I 6. A valved'line I7 continuously fed digestion liquor over the material being extruded and a valved line I8 continuously fed steam under the material. The digestion liquor was the same as the solution used in prctrcatment zone except that it was heated to about 340o and continuously charged in a ratio of 2 parts of liquor to 1 part of linters. if desired, as little as l part of liquor to each part of linters can be used. The valVed line I8 was adjusted to a steam pressure of pounds. The digestion zone I6 was composed of a plurality of digesters represented by IB in superposed relationship. Each digester was provided with a driven screw conveyor represented by 20 which agitated and progressed the material substantially throughout the length of the digester. The rst digester' progressed the material in one direction and its subjacent digester in the opposite direction and so forth throughout the digestion zone it. rEhe conveyors were .interconnected and uniformly driven by a motor 2| and the digesters were connected to each other by conduits represented by 22. A pressure and temperature recorder was provided for determining the pressure and temperature within the digester at Various points. The material was in the digestion zone iii for approximately 12 minutes at an average temperature of about 338. The material from the digestion zone I6 was then passed through a conduit 23 into a second compaction zone 2d in which a major portion of the spent digestion liquor was removed as the material was formed into a compact. The compaction Zone 24 contained a motor-driven screw 25 disposed in a foraminous jacket 26 through which the excess liquor passed as the material was compacted by the screw. The excess liquor was removed from the compaction Zone 24 through conduit 2'! into black liquor tank 28 as the material was continuously formed into the compact by being forced against a pressure-actuated ram 2t. The ram 29 was provided with a valved air line et for controlling the amount of force delivered by the ram against the compact and for controlling the amount of black liquor removed during compaction. The material was continuously extruded 29 where it was disintegrated by the continuous and directly opposed compressive force and dropped therefrom to the bottom of a pressureequalizing Zone 3|. 'I'he zone 3I was maintained at approximately the same pressure as that in the digestion zone I6 by line 32. The material Afrom zone 3l passed through a conduit 33 into a blow tank 34 which in turn discharged the material into a receiving tank 35. A blow valve 36 within the blow tank 34 was intermittently actuated at ten-second intervals by an air line 31 whereby the material was blown into the receiving tank 35 at substantially atmospheric pressure. rIhe time interval during which the blow valve 3S was open was regulated so that the pressure drop did not exceed 5 pounds. The formerly compacted material was found to be thoroughly disintegrated at this stage of the process. An agitator 38 was provided in the receiving tank 35 and the slurry therein continuously agitated. The steam and vapor accumulating within the receiving tank 35 were vented to the atmosphere through line 39 and the slurry was continuously withdrawn. Waste water from a washer (not shown) was continuously admitted by line 43 to the receiving tank 3E and the slurry was maintained at a ratio of about v49 parts of waste water to about 1 part material. From the bottom of the tank 35, the slurry was pumped through line 4I to suitable equipment (not shown) wherein it was washed and subsequently bleached using conventional procedure. rlhe resulting product possessed good quality and exu cellent uniformity.

2 is an enlarged view of compact disintegrating zone 43 and associated apparatus necessary for the disintegration of the pressure-resistant compact of cellulosic material. Figs. 3, a, 5, and 6 depict various stages in the formation and disintegration of the pressure-resistant compact, and these latter figures will be discussed in conjunction with a discussion of Fig. 2.

The cellulosic material wetted with pretreatment liquid is extruded through compacting zone It by screw I I, and the compact then passes via conduit 42 into zone 43. In zone 43 the compact contacts pressure-actuated ram I4, and in the initial stage'of the contacting the compact and ram are in a position similar to that shown in Fig. 3. The pressure exerted upon ram I4 by the air in line I5 causes ram I4 to exert a force against the compact, but in the initial stage, as shown in Fig. 3, the internal cohesive force of the compact is greater than the forces exerted upon it by screw II and ram I4. Consequently, the movement of screw l I and the continued formation and increase in length of compact causes a backward movement of ram I4 into a position such as that shown in Fig. 4. In Fig.v 4 the internal cohesive force of the compact is about equal to or slightly greater than the forces exerted on it by screw II and ram I4. However, as the movement of screw II continues, the length of the compact increases, and the compact begins to bulge convexly and to cripple and fracture as shown in Fig. 5. The compact then disintegrates or is comminuted into many small fragments of cellulosic material and upon disintegration of the compact, ram I4 moves forward quickly into contact with an unbroken or unfractured portion of the compact, as shown in Fig. 1. Further formation and successive disintegration of the compact is then effected in the manner described.

If the compact of cellulosic material formed by screw IIV should fail either inside or outside zone 43, ram I4 acts as a check valve against the prese sure within digestion zone I B. Upon failure of the compact, ram I4 quickly moves forward to seal the opening through which the compact enters zone 43 after passage through conduit 42. During satisfactory operation and formation of the compact, the compact itself acts to maintain the pressure within digestion zone I5, and, upon failure of the compact, ram I4 seals the opening in the manner described above.

The above description of the procedure and apparatus for forming and disintegrating a pressure-resistant compact has been directed primarily to zone 43, but a similar procedure and apparatus are employed in zone 3l.

rihe facing or extremity of rams I4 and 29 adjacent the compact of cellulosic material can be flat, as in Figs. 3, 4, 5 and 6, or it can be curved convexly, as shown in Figs. 1 and 2. In some instances the convex curvature is preferred in order to obtain a more eective seal in the event of failure of the compact of cellulosic material.

The pressure that is exerted on the ram through the suitably disposed pressure line can be either constant or varying. When a varying pressure is used, the pressure ordinarily is increased as the ram is forced backwardly by the extruding screw and compact.

It is evident that there are numerous factors which will influence conditions for the most satisfactory operation of the invention, the actual limits of which cannot be determined except by a detailed study of each set of raw materials and the finished product involved. For example, in another embodiment of the invention, the material from the digestion zone may be charged directly into the pressure-equalizing zone. In instances where the consistency is maintained at a high level and there is little or substantially no excess liquor present, the material may be passed directly into the pressure-equalizing zone. The raw material may be a cellulosic material such as wood chip, wood waste, wheat straw and other agricultural residues, linters, and pulps requir ing further refinement. The raw material may be dibrated prior to digestion or subsequent to digestion as desired. The pretreatment liquid may be chemically inert such as water, or may be a chemically active aqueous solution containing chlorine, sodium sulfide and hydroxide, sulfurous acid and a bisulte, sodium hydroxide, and the like. It will be seen, therefore, that the pretreatment liquid may be water per se, or bleach solution such as aqueous hypochlorite, or digestion solution such as aqueous sodium hydroxide. The digestion liquid may be an aqueous solution of any of the chemically active agents hereinbefore referred to for pretreatment depending on the raw material involved. Generally, the quantity and type of chemicals used, the pressure and temperature, and length of the digestion period may be varied according to the yield and quality of the cellulose desired. In accordance with the preferred embodiment of this invention, wherein the raw material is cotton linters, the pretreatment liquid may range from a weak to a strong aqueous solution of caustic alkali, that is, from about 0.5 to about '7 and higher, say, up to 15%, depending on the quality of the starting material and quality of the cellulose desired. The digestion liquor may be an aqueous solution comprising from about 0.5 to about 10% caustic alkali with digestion carried out under a steam pressure from about 25 to about 175 pounds gage per square inch at a temperature from about 266 f! to about 377 F. During digestion, the ratio of digestion liquor to linters may be maintained from about 1:1 to about 5:1 with satisfactory operation, and from the standpoint of economy the lowest possible liquor to linters ratio, say, approaching a 1:1 ratio, is used. Detergente, wetting agents, and other digestion aids may be added to the digestion liquor or added to the digester to aid in the removal of undesirable material during digestion. Similarly, in the suliite, soda, and sulfate processes which constitute the major proportion of chemical pulps, conventional digestion chemicals and moderants may be utilized in conjunction with this invention with distinct benet. This is more readily seen in reference to the advantages of the invention. For example, the pretreatment step affords thorough wetting and necessary lubrication for charging the material and may include some chemical action if desired. It has been pointed out above that a low liquor to linters ratio is desirable for economic reasons, and it is possible to use far lower ratios in this continuous process than in batch digestion procedures. The main reason for this improvement is the thorough and uniform distribution of a small amount of liquor through the mass of linters that is accomplished by the action of the charging screw in squeezing out excess liquor. Additionally, excess solution is removed which from the standpoint of chemical recovery is important throughout the entire process. The heat distribution and Contact of the material with chemical throughout the digestion step is exceptionally uniform and thorough so that low liquor to linters ratios increased chemical concentration and reduced time of digestion may be employed. Additionally,

chemical concentration may be varied through` out the digestion zone by providing intermediate points along the digesters for charging dilution or concentration medium to the zone as desired. Excess solution, if present, is removed from the digested material so that the chemicals can be recovered or reused before being diluted with copious amounts of water which entail additional expense in recovery or" chemical or concentration for reuse. The digested material in this relatively dry and pressurized state is blown to substantially atmospheric pressure at intermittent intervals. rFhis sudden expulsion distends the material and renders it ideal for subsequent treatment including washing, bleaching, debration, r similar desired after-treatment procedures.

It will be seen, therefore, that the advantages of this invention are multifold and that the invention may be carried out by the use of various modincations and changes without departinfr from its spirit and scope.

What I claim and desire to protect by Letters Patent is:

1. The method for forming and disintegrating a pressure-resistant compact of cellulosic material which comprises continuously forming a pressure-resistent compact of ceilulosic material containing liquid in a conduit by extruding said material against a pressure-actuated ram, and successively disintegrating the compact so formed by continuously extruding said compact from the conduit as an integral body of sufficient strength to force the ram backward with continued lengthening of said body to a point at which a substantial portion of the entire length of said body of material is instantly disintegrated into fragments by the compressive force exerted thereon between the conduit and the ram after which said ram moves forward to engage a new portion of the compact being continuously extruded from the conduit and the operation repeats to give successive disintegration of the continuously formed pressure-resistant compact.

2. The method for forming and disintegrating a pressure-resistant compact of cellulosic material which comprises continuously forming a pressure-resistant compact 0f wet cellulosic material and removing liquid therefrom in a conduit by extruding said material against a pressure-actuated ram, and successively disintegrating the compact so formed by continuously extruding said compact from the conduit as an integral body of sufiicient strength to force the ram backward with continued lengthening of said body to a point at which a substantial portion of the entire length of said body of material is instantly disintegrated into fragments by the compressive force exerted thereon between the conduit and the ram after which said ram moves forward to engage a new portion of the compact being continuously extruded from the conduit and the operation repeats to give successive disintegration of the continuously formed pressure-resistant compact.

3. The method for forming and disintegrating a pressure-resistant compact of cellulosic material which comprises continuously forming a pressure-resistant compact of wet cellulosic material and removing liquid therefrom in a conduit by extruding said material Vagainst a pressure-actuated ram. successively disintegrating the compact so formed by continuously extruding said compact from the conduit as an integral body of sufcient strength to force the ram backward with continued lengthening of said body to a point at which a substantial portion of the entire length of said body of material is instantly disintegrated into fragments by the compressive force exerted thereon between the conduit and the ram after which said, ram moves forward to engage a new portion of the compact being con tinuously extruded from the conduit and the operation repeats to give successive disintegration of the continuously formed pressure-resistant compact, and discharging the material thus disintegrated into a zonev maintained at a pressure other than atmospheric, said zone being in communication with the exit end of the conduit.

4. The method for forming and disintegrating a pressure-resistant compact of cellulosic material which comprises continuously forming a pressure-resistant compact of wet cellulosic material and removing liquid therefrom in a conduit by extruding said material against a pressure-actuated ram, successively disintegrating the compact so formed by continuously extruding said compact from the conduit as an integral body or sufcient strength to force the ram backward with continued lengthening of said body to a point at which a substantial portion of the entire length of said body of material is instantly disintegrated into fragments by the compressive force exerted thereon between the conduit and the ram after which said ram moves forward to engage a new portion of the compact being continuously extruded from the conduit and the operation repeats to give successive disintegration of the continuously formed pressure-resistant compact, and discharging the material thus disintegrated into a zone maintained at a pressure other than atmospheric, said zone being in communication with ,the kexit `end of the 9 conduit and the ram being sealable to said exit end of the conduit in the event of failure of the compact within the conduit.

5. The method in accordance with claim 1 in which the cellulosic material is cotton linters.

6. The method in accordance with claim 1 in which the cellulosic lmaterial is wood chip.

7. The method in accordance with claim 1 in which the celluiosic material is wood waste.

8. The method in accordance with claim 1 in which the cellulosic material is Wheat straw.

9. The method in accordance with claim 1 in which the cellulosic material is pulp requiring further refinement.

WALTER E. SEGL.

References Cited in the le of this patent UNITED STATES PATENTS Number 

